Encapsulated perfume particles and detergent compositions containing said particles

ABSTRACT

Modified starch encapsulated High Impact Accord (HIA) perfume particles are disclosed. The particles consist of a modified starch and perfume oil encapsulated by the starch and comprised of at least two HIA perfume ingredients which have a boiling point at 760 mm Hg, of 275° C. of lower, a calculated ClogP of 2.0 or higher, and an odor detection threshold less than or equal to 50 parts per billion (ppb). The encapsulated perfume particles are particularly useful in laundry compositions.

This application claims the benefit of provisional application No.60/082,725, filed Apr. 23, 1998.

FIELD OF THE INVENTION

The present invention relates to encapsulated perfume particles,especially for delivery of high impact accord (HIA) perfume ingredients,and detergent compositions comprising these encapsulated perfumeparticles, especially granular detergents.

BACKGROUND OF THE INVENTION

Most consumers have come to expect scented detergent products and toexpect that fabrics and other items which have been laundered with theseproducts also have a pleasing fragrance. In many parts of the worldhandwashing is the predominant means of laundering fabrics. Whenhandwashing soiled fabrics the user often comes in contact with the washsolution and is in close proximity to the detergent product usedtherein. Handwash solutions may also develop an offensive odor uponaddition of soiled clothes. Therefore, it is desirable and commerciallybeneficial to add perfume materials to such products. Perfume additivesmake laundry compositions more aesthetically pleasing to the consumer,and in some cases the perfume imparts a pleasant fragrance to fabricstreated therewith. However, the amount of perfume carryover from anaqueous laundry bath onto fabrics is often marginal. Industry,therefore, has long searched for an effective perfume delivery systemfor use in detergent products which provides long-lasting,storage-stable fragrance to the product, as well as fragrance whichmasks wet solution odor during use and provides fragrance to thelaundered items.

Detergent compositions which contain perfume mixed with or sprayed ontothe compositions are well known from commercial practice. Becauseperfumes are made of a combination of volatile compounds, perfume can becontinuously emitted from simple solutions and dry mixes to which theperfume has been added. Various techniques have been developed to hinderor delay the release of perfume from compositions so that they willremain aesthetically pleasing for a longer length of time. To date,however, few of the methods deliver significant fabric and wet solutionodor benefits after prolonged storage of the product.

Moreover, there has been a continuing search for methods andcompositions which will effectively and efficiently deliver perfume intoan aqueous laundry bath providing a relatively strong scent in theheadspace just above the solution, then from the laundry bath ontofabric surfaces. Various methods of perfume delivery have been developedinvolving protection of the perfume through the wash cycle, withsubsequent release of the perfume onto fabrics.

One method for delivery of perfume in the wash cycle involves combiningthe perfume with an emulsifier and water- soluble polymer, forming themixture into particles, and adding them to a laundry composition, as isdescribed in U.S. Pat. No. 4,209,417, Whyte, issued Jun. 24, 1980; U.S.Pat. No. 4,339,356, Whyte, issued Jul. 13, 1982; and U.S. Pat. No.3,576,760, Gould et al, issued Apr. 27, 1971. However, even with thesubstantial work done by industry in this area, a need still exists fora simple, more efficient and effective perfume delivery system which canbe mixed with laundry compositions to provide initial and lastingperfume benefits to fabrics which have been treated with the laundryproduct.

Another problem in providing perfumed products is the odor intensityassociated with the products, especially high density granular detergentcompositions. As the density and concentration of the detergentcomposition increase, the odor from the perfume components can becomeundesirably intense. A need therefore exists for a perfume deliverysystem which substantially releases the perfume odor during use andthereafter from the dry fabric, but which does not provide anoverly-intensive odor to the product itself.

By the present invention it has now been discovered that perfumeingredients, can be selected based on specific selection criteria tomaximize impact during and/or after the wash process, while minimizingthe amount of ingredients needed in total to achieve a consumernoticeable benefit. Such compositions are desirable not only for theirconsumer noticeable benefits (e.g., odor aesthetics), but also for theirpotentially reduced cost through efficient use of lesser amounts ofingredients.

The present invention solves the long-standing need for a simple,effective, storage-stable delivery system which provides surprising odorbenefits (especially wet solution odor benefits) during and after thelaundering process. Further, encapsulated perfume-containingcompositions have reduced product odor during storage of thecomposition.

SUMMARY OF THE INVENTION

The present invention relates to modified starch encapsulated HighImpact Accord (“HIA”) perfume particles; said particles comprising amodified starch and HIA perfume oil comprised of at least two HIAperfume ingredients which have a boiling point at 760 mm Hg, of 275° C.or lower, a calculated CLogP of 2.0 or higher, and an odor detectionthreshold less than or equal to 50 parts per billion (ppb), wherein theperfume ingredients are encapsulated with the modified starch.

The present invention further relates to laundry compositions comprisingfrom about 0.01% to 50% (preferably from about 0.05% to 8.0%; morepreferably from about 0.05% to 3.0% and most preferably from about 0.05to 1.0%) of a perfume particle according to the present invention and intotal from about 50% to about 99.99% preferably from about 92% to99.95%; more preferably from about 97% to 99.95% and most preferablyfrom about 99% to 99.95%) of conventional laundry ingredients selectedfrom the group consisting of surfactants, builders, bleaching agents,enzymes, soil release polymers, dye transfer inhibitors, fillers andmixtures thereof.

All percentages, ratios, and proportions herein are on a weight basisunless otherwise indicated. All documents cited are hereby incorporatedby reference in their entirety.

DETAILED DESCRIPTION OF THE INVENTION

The present invention provides perfumed, dry particulate detergentcompositions useful for the washing of fabrics having an especiallydesirable and noticeable odor attributable to a modified starchencapsulated HIA perfume particle. The HIA perfume oil contains at leasttwo HIA perfume ingredients. An HIA perfume ingredient has a boilingpoint at 760 mm Hg, of 275° C. or lower, a calculated log₁₀ of itsoctanol/water partition coefficient, P, of about 2 or higher and an odordetection threshold less than or equal to 50 ppb.

The HIA perfume ingredients are selected according to specific selectioncriteria described in detail hereinafter. The selection criteria furtherallow the formulator to take advantage of interactions between theseagents when incorporated into the modified starch encapsulate tomaximize consumer noticeable benefits while minimizing the quantities ofingredients utilized.

It is also preferable to use both free perfume and encapsulated perfumein the same particulate detergent composition, with the two perfumesbeing either the same, or two different perfumes. Normally, the freeperfume provides the product (or container) perfume fragrance, andcovers any base product odor, while the encapsulated perfume providesthe in-use perfume odor when the detergent composition is diluted intothe wash water.

HIA Perfume Oil

The HIA perfume oil comprises HIA perfume ingredients. An HIA perfumeingredient is characterized by its boiling point (B.P.), itsoctanol/water partition coefficient (P) and its odor detection threshold(“ODT”). The octanol/water partition coefficient of a perfume ingredientis the ratio between its equilibrium concentrations in octanol and inwater. An HIA perfume ingredient of this invention has a B.P.,determined at the normal, standard pressure of about 760 mm Hg, of about275° C. or lower, an octanol/water partition coefficient P of about2,000 or higher, and an ODT of less than or equal to 50 parts perbillion (ppb). Since the partition coefficients of the preferred perfumeingredients of this invention have high values, they are moreconveniently given in the form of their logarithm to the base 10, logP.Thus the preferred perfume ingredients of this invention have logP ofabout 2 and higher.

The boiling points of many perfume ingredients, at standard 760 mm Hgare given in, e.g., “Perfume and Flavor Chemicals (Aroma Chemicals),”Steffen Arctander, published by the author, 1969, incorporated herein byreference.

The logP values of many perfume ingredients have been reported; forexample, the Pomona92 database, available from Daylight ChemicalInformation Systems, Inc. (Daylight CIS), Irvine, Calif., contains many,along with citations to the original literature. However, the logPvalues are most conveniently calculated by the “CLOGP” program, alsoavailable from Daylight CIS. This program also lists experimental logPvalues when they are available in the Pomona92 database. The “calculatedlogP” (ClogP) is determined by the fragment approach of Hansch and Leo(cf., A. Leo, in Comprehensive Medicinal Chemistry, Vol. 4, C. Hansch,P. G. Sammens, J. B. Taylor and C. A. Ramsden, Eds., p. 295, PergamonPress, 1990, incorporated herein by reference). The fragment approach isbased on the chemical structure of each perfume ingredient, and takesinto account the numbers and types of atoms, the atom connectivity, andchemical bonding. The ClogP values, which are the most reliable andwidely used estimates for this physicochemical property, are preferablyused instead of the experimental logP values in the selection of perfumeingredients which are useful in the present invention.

Odor detection thresholds are determined using a gas chromatograph. Thegas chromatograph is calibrated to determine the exact volume ofmaterial injected by the syringe, the precise split ratio, and thehydrocarbon response using a hydrocarbon standard of known concentrationand chain-length distribution. The air flow rate is accurately measuredand, assuming the duration of a human inhalation to last 12 seconds, thesampled volume is calculated. Since the precise concentration at thedetector at any point in time is known, the mass per volume inhaled isknown and hence the concentration of material. To determine whether amaterial has a threshold below 50 ppb, solutions are delivered to thesniff port at the back-calculated concentration. A panelist sniffs theGC effluent and identifies the retention time when odor is noticed. Theaverage across all panelists determines the threshold of noticeability.

The necessary amount of analyte is injected onto the column to achieve a50 ppb concentration at the detector. Typical gas chromatographparameters for determining odor detection thresholds are listed below.

GC: 5890 Series II with FID detector

7673 Autosampler

Column: J&W Scientific DB-1

Length 30 meters ID 0.25 mm film thickness 1 micron

Method:

Split Injection: 17/1 split ratio

Autosampler: 1.13 microliters per injection

Column Flow: 1.10 mL/minute

Air Flow: 345 mL/minute

Inlet Temp. 245° C.

Detector Temp. 285° C.

Temperature Information

Initial Temperature: 50° C.

Rate: 5C/minute

Final Temperature: 280° C.

Final Time: 6 minutes

Leading assumptions:

(i) 12 seconds per sniff

(ii) GC air adds to sample dilution

An HIA perfume oil is composed of at least two HIA perfume ingredients,each HIA perfume ingredient having:

(1) a standard B.P. of about 275° C. or lower at 760 mm Hg, and;

(2) a ClogP, or an experimental logP, of about 2 or higher, and;

(3) an ODT of less than or equal to 50ppb and greater than 10 ppb,

and is encapsulated in a modified starch as described hereinafter, andused in a particulate detergent cleaning composition. The HiA perfumeoil is very effusive and very noticeable when the product is in use aswell as on fabric items that come in contact with the wash solution. Ofthe perfume ingredients in a given perfume oil, at least 40%, preferablyat least 50% and most preferably at least 70% are HIA perfumeingredients.

Table 1 gives some non-limiting examples of HIA perfume ingredients.

TABLE 1 HIA Perfume Ingredients HIA Ingredient4-(2,2,6-Trimethylcyclohex-1-enyl)-2-en-4-one 2,4-Decadienoic acid,ethyl ester (E,Z)- 6-(and -8) isopropylquinoline Acetaldehydephenylethyl propyl acetal Acetic acid, (2-methylbutoxy)-, 2-propenylester Acetic acid, (3-methylbutoxy)-, 2-propenyl ester2,6,10-Trimethyl-9-undecenal Glycolic acid, 2-pentyloxy-, allyl esterHexanoic acid, 2-propenyl ester 1-Octen-3-ol trans-Anethole iso buthyl(z)-2-methyl-2-butenoate Anisaldehyde diethyl acetal Benzenepropanal,4-(1,1-dimethylethyl)- 2,6-Nonadien-1-ol3-methyl-5-propyl-cyclohexen-1-onre Butanoic acid, 2-methyl-, 3-hexenylester, (Z)- Acetaldehyde, [(3,7-dimethyl-6-octenyl)oxy]- Lauronitrile2,4-dimethyl-3-cyclohexene-1-carbaldehyde 2-Buten-1-one,1-(2,6,6-trimethyl-1,3-cyclohexadien-1-yl)- 2-Buten-1-one,1-(2,6,6-trimethyl-2-cyclohexen-1-yl)-, (E)- gamma-Decalactonetrans-4-decenal decanal 2-Pentylcyclopentanone 1-(2,6,6 Trimethyl 3Cyclohexen-1-yl)-2 Buten-1-one) 2,6-dimethylheptan-2-ol Benzene,1,1′-oxybis- 4-Penten-1-one, 1-(5,5-dimethyl-1-cyclohexen-1-yl)-Butanoic acid, 2-methyl-, ethyl ester Ethyl anthranilate2-Oxabicyclo[2.2.2]octane, 1,3,3-trimethyl- Eugenol3-(3-isopropylphenyl)butanal methyl 2-octynoate4-(2,6,6-trimethyl-1-cyclohexen-1-yl_-3-buten-2-one Pyrazine,2-methoxy-3-(2-methylpropyl)- Quiniline, 6-secondary buty Isoeugenol2H-Pyran-2-one, tetrahydro-6-(3-pentenyl)- Cis-3-Hexenyl MethylCarbonate Linalool 1,6,10-Dodecatriene, 7,11-dimethyl-3-methylene-, (E)-2,6-dimethyl-5-heptenal 4,7 Methanoindan 1-carboxaldehyde, hexahydro2-methylundecanal methyl 2-nonynonate1,1-dimethoxy-2,2,5-trimethyl-4-hexene Benzoic acid, 2-hydroxy-, methylester 4-Penten-1-one, 1-(5,5-dimethyl-1-cyclohexen-1-yl) 2H-Pyran,3,6-dihydro-4 methyl-2-(2-methyl-1-propenyl)- 2,6-Octadienenitrile,3,7-dimethyl-, (Z)- 2,6-nonadienal 6-Nonenal, (Z)- nonanal octanal2-Nonenenitrile Acetic acid, 4-methylphenyl ester Gamma Undecalactone2-norpinene-2-propionaldehyde 6,6 dimethyl 4-nonanolide 9-decen-1-ol2H-Pyran, tetrahydro-4-methyl-2-(2-methyl-1-propenyl)-5-methyl-3-heptanone oxime Octanal, 3,7-dimethyl- 4-methyl-3-decen-5-ol10-Undecen-1-al Pyridine, 2-(1-ethylpropyl)-Spiro[furan-2(3H),5′-[4,7]methano[5H]indene], decahydro-

The following are non-limiting examples of suitable perfume oilcompositions for use in the present invention:

EXAMPLE 1

HIA Perfume Ingredient Conc. Boiling Point Trade Name Wt. % ODT ° C.ClogP Eugenol  5 <50 PPB 259 2.4 Lilial 15 <50 PPB 280 3.9 Linalool 25<50 PPB 197 3.0 beta-Naphthyl methyl ether  5 <50 PPB 270 3.2 AnisicAldehyde 10 <50 PPB 249 2.0 Flor Acetate 10 <50 PPB 265 2.4 Ionone Beta10 <50 PPB 265 3.8 Rose Oxide 10 <50 PPB 201 2.9 Damascenone  5 <50 PPB260 4.3 Cyclal C  5 <50 PPB 199 2.4 Total 100 

EXAMPLE 2

HIA Perfume Ingredient Conc. Boiling Point Trade Name Wt. % ODT ° C.ClogP Cyclal C 10 <50 PPB 199 2.4 Damascone Alpha  5 <50 PPB 255 4.7Rose Oxide 10 <50 PPB 201 2.9 Ionone Beta 25 <50 PPB 265 3.8Cis-3-Hexenyl Salycilate 15 <50 PPB 271  4.84 Methyl Octine Carbonate  5<50 PPB 219 3.1 Lilial 30 <50 PPB 280 3.9 Total 100 

EXAMPLE 3

HIA Perfume Ingredient Conc. Boiling Point Trade Name Wt. % ODT ° C.ClogP Damascone Alpha  5 <50 PPB 255 4.7 Cyclal C  5 <50 PPB 199 2.4Rose Oxide 10 <50 PPB 201 2.9 Ionone Beta 25 <50 PPB 265 3.8 Frutene 15<50 PPB 275 2.9 Anisic Aldehyde 10 <50 PPB 249 2.0 Ethyl-2-methylButyrate  5 <50 PPB 129 2.1 Lilial 25 <50 PPB 280 3.9 Total 100 

Encapsulating Material

The HIA perfume oils are encapsulated with a water soluble, modifiedstarch to form the modified starch encapsulate. Encapsulation of the HIAperfume oils in the water soluble modified starch provides an enhancedfragrance signal during use, when used in detergent compositions.

Starches suitable for encapsulating the perfume oils of the presentinvention can be made from, raw starch, pregelatinized starch, modifiedstarch derived from tubers, legumes, cereal and grains, for example cornstarch, wheat starch, rice starch, waxy corn starch, oat starch, cassavastarch, waxy barley, waxy rice starch, sweet rice starch, amioca, potatostarch, tapioca starch, oat starch, cassava starch, and mixturesthereof.

Modified starches suitable for use as the encapsulating matrix in thepresent invention include, hydrolyzed starch, acid thinned starch,starch esters of long chain hydrocarbons, starch acetates, starchoctenyl succinate, and mixtures thereof.

The term “hydrolyzed starch” refers to oligosaccharide-type materialsthat are typically obtained by acid and/or enzymatic hydrolysis ofstarches, preferably corn starch. Suitable hydrolyzed starches forinclusion in the present invention include maltodextrins and corn syrupsolids. The hydrolyzed starches for inclusion with the mixture of starchesters have a Dextrose Equivalent (DE) values of from about 10 to about36 DE. The DE value is a measure of the reducing equivalence of thehydrolyzed starch referenced to dextrose and expressed as a percent (ona dry basis). The higher the DE value, the more reducing sugars present.A method for determining DE values can be found in Standard AnalyticalMethods of the Member Companies of Corn Industries Research Foundation,6th ed. Corn Refineries Association, Inc. Washington, D.C. 1980, D-52.

Starch esters having a degree of substitution in the range of from about0.01% to about 10.0% may be used to encapsulate the perfume oils of thepresent invention. The hydrocarbon part of the modifying ester should befrom a C₅ to C₁₆ carbon chain. Preferably, octenylsuccinate (OSAN)substituted waxy corn starches of various types such as 1) waxy starch:acid thinned and OSAN substituted, 2) blend of corn syrup solids: waxystarch, OSAN substituted, and dextrinized, 3) waxy starch: OSANsubstituted and dextrinized, 4) blend of corn syrup solids ormaltodextrins with waxy starch: acid thinned OSAN substituted, and thencooked and spray dried, 5) waxy starch: acid thinned and OSANsubstituted then cooked and spray dried, and 6) the high and lowviscosities of the above modifications (based on the level of acidtreatment) can also be used in the present invention.

Modified starches having emulsifying and emulsion stabilizing capacitysuch as starch octenyl succinates have the ability to entrap the perfumeoil droplets in the emulsion due to the hydrophobic character of thestarch modifying agent. The perfume oils remain trapped in the modifiedstarch until dissolved in the wash solution, due to thermodynamicfactors i.e., hydrophobic interactions and stabilization of the emulsionbecause of steric hindrance.

EXAMPLE 4 Manufacture of Modified Starch Encapsulated HIA PerfumeParticles

The following is a non-limiting example of a suitable process formanufacture of a modified starch encapsulated HIA perfume particle foruse in detergent compositions according to the present invention.

1. 225 g of CAPSUL modified starch (National Starch & Chemical) is addedto 450 g of water at 24° C.

2. The mixture is agitated at 600 RPM (turbine impeller 2 inches indiameter) for 20 minutes.

3. 75 g perfume oil is added near the vortex of the starch solution.

4. The emulsion formed is agitated for an additional 20 minutes (at 600RPM).

5. Upon achieving a perfume droplet size of less than 15 microns, theemulsion is pumped to a spray drying tower and atomized through aspinning disk with co-current airflow for drying. The inlet airtemperature is set at 205-210° C., the exit air temperature isstabilized at 98-103° C.

6. Dried particles of the starch encapsulated perfume oil are collectedat the dryer outlet.

Analysis of the finished HIA perfume particle (all % based on weight):

Total Perfume Oil 24.56% Encapsulated Oil 24.46% Free/Surface Oil 0.10%Starch 72.57% Moisture 2.87% Particle Size Distribution <50 micrometers16% 50-500 micrometers 83% >500 micrometers 1%

Other known methods of manufacturing the starch encapsulates of thepresent invention, include but are not limited to, fluid bedagglomeration, extrusion, cooling/crystallization methods and the use ofphase transfer catalysts to promote interfacial polymerization.

When a detergent composition containing the encapsulated HIA perfumeparticles described herein is added to water the modified starch of theperfume particles begins to dissolve in the water. Not wishing to bebound by theory it is believed that the dissolving modified starchswells and an emulsion of perfume droplets, modified starch and water isformed, the modified starch being the emulsifier and emulsionstabilizer. After the emulsion is formed, the perfume oil begins tocoalesce into larger droplets of perfume, which can migrate to eitherthe surface of the solution or to the surface of fabrics in the washsolution due to the relative density difference between the perfumedroplets (mostly low density hydrophobic oils) and the wash water. Whenthe droplets reach either interface, they spread out quickly along thesurface or interface. The spreading of the perfume droplet at the washsurface increases the surface area from which the perfume oil canvolatilize, thereby releasing larger amounts of the perfume into theheadspace above the wash solution. This provides a surprisingly strongand consumer noticeable scent in the headspace above the wash solution.When an equal mass of HIA perfume oil is delivered in a granulardetergent via HIA particles according to the present invention asopposed to being sprayed on or delivered via cyclodextrin capsules themass of perfume present in the headspace above the wash solution is tenfold greater. This can be confirmed by collection of the headspace air,from which the delivered perfume is subsequently condensed and its massdetermined using conventional gas chromatography. Furthermore, theinteraction of the perfume droplets with wet fabrics in solutionprovides a surprisingly strong and consumer noticeable scent on wet anddry fabrics.

Encapsulation of the HIA perfume oils as described above allows forloading of larger amounts of perfume oil than if they were encapsulatedin a native starch granule. Encapsulation of perfume oils usingcylodextrin is limited by the particle size of the guest molecule(perfume) and the cavity of the host (cyclodextrin). It is difficult toload more than about 20% perfume into a cyclodextrin particle. However,encapsulation with a starch that has been modified to have emulsionproperties does not impose this limitation. Since the encapsulation inthe present invention is achieved by entrapping perfume oil droplets ofless than 15 microns, preferably less than 5 microns and most preferablyless than 2.5 microns in size, within the modified starch matrix, whilethe matrix is being formed by removal of water from the emulsion, moreperfume can be loaded based on the type, method and level ofmodification of the starch. In contrast, traditional cyclodextrinmolecules trap the perfume oil completely inside their cavity therebylimiting the size and amount of the perfume oil encapsulated. Loads muchgreater than 20% are possible when encapsulating with the modifiedstarches described by this invention.

Encapsulation of the volatile HIA perfume oils also minimizes depletionduring storage and when the product container is opened. Further, HIAperfumes are generally only released when detergents containing theencapsulated particle are dissolved in the wash solution. Furthermore,the water soluble encapsulating matrix protects the perfume oil fromchemical degradation caused in the neat product as well as in the washsolution, by the different surfactant systems or bleaches which arecommonly present in the particulate detergent compositions of thisinvention.

Other suitable matrix materials and process details are disclosed in,e.g., U.S. Pat. No. 3,971,852, Brenner et al., issued Jul. 27, 1976,which is incorporated herein by reference.

Water soluble perfume microcapsules containing conventional, non-HIAperfume oils can be obtained commercially, e.g., as IN-CAP® from Polak'sFrutal Works, Inc., Middletown, N.Y.; and as Optilok System®encapsulated perfumes from Encapsulated Technology, Inc., Nyack, N.Y.

The detergent compositions herein comprise from about 0.01% to 50% ofthe above described modified starch encapsulated HIA perfume particle.More preferably, the detergent compositions herein comprise from about0.05% to 8.0% of the HIA perfume particle, even more preferably fromabout 0.5% to 3.0%. Most preferably, the detergent compositions hereincontain from about 0.05% to 1.0% of the encapsulated HIA perfumeparticle. The encapsulated perfume particles preferably have size offrom about 1 micron to about 1000 microns, more preferably from about 50microns to about 500 microns.

The encapsulated perfume particles are used in compositions withdetersive ingredients, as follows.

Optional Detersive Adjuncts

As a preferred embodiment, the conventional detergent ingredients areselected from typical detergent composition components such as detersivesurfactants and detersive builders. Optionally, the detergentingredients can include one or more other detersive adjuncts or othermaterials for assisting or enhancing cleaning performance, treatment ofthe substrate to be cleaned, or to modify the aesthetics of thedetergent composition. Usual detersive adjuncts of detergentcompositions include the ingredients set forth in U.S. Pat. No.3,936,537, Baskerville et al. and in Great Britain Patent ApplicationNo. 9705617.0, Trinh et al., published Sep. 24, 1997. Such adjuncts areincluded in detergent compositions at their conventional art-establishedlevels of use, generally from 0% to about 80% of the detergentingredients, preferably from about 0.5% to about 20% and can includecolor speckles, suds boosters, suds suppressors, antitarnish and/oranticorrosion agents, soil-suspending agents, soil release agents, dyes,fillers, optical brighteners, germicides, alkalinity sources,hydrotropes, antioxidants, enzymes, enzyme stabilizing agents, solvents,solubilizing agents, chelating agents, clay soilremoval/anti-redeposition agents, polymeric dispersing agents,processing aids, fabric softening components, static control agents,bleaching agents, bleaching activators, bleach stabilizers, etc.

Granular Detergent Composition

The encapsulated perfume particles hereinbefore described can be used inboth low density (below 550 grams/liter) and high density granulardetergent compositions in which the density of the granule is at least550 grams/liter or in a laundry detergent additive product. Such highdensity detergent compositions typically comprise from about 30% toabout 90% of detersive surfactant.

Low density compositions can be prepared by standard spray- dryingprocesses. Various means and equipment are available to prepare highdensity granular detergent compositions. Current commercial practice inthe field employs spray-drying towers to manufacture granular laundrydetergents which often have a density less than about 500 g/l.Accordingly, if spray drying is used as part of the overall process, theresulting spray-dried detergent particles must be further densifiedusing the means and equipment described hereinafter. In the alternative,the formulator can eliminate spray-drying by using mixing, densifyingand granulating equipment that is commercially available.

High speed mixer/densifiers can be used in the present process. Forexample, the device marketed under the trademark “Lodige CB30” Recyclercomprises a static cylindrical mixing drum having a central rotatingshaft with mixing/cutting blades mounted thereon. Other such apparatusincludes the devices marketed under the trademark “Shugi Granulator” andunder the trademark “Drais K-TTP 80”. Equipment such as that marketedunder the trademark “Lodige KM600 Mixer” can be used for furtherdensification.

In one mode of operation, the compositions are prepared and densified bypassage through two mixer and densifier machines operating in sequence.Thus, the desired compositional ingredients can be admixed and passedthrough a Lodige mixture using residence times of 0.1 to 1.0 minute thenpassed through a second Lodige mixer using residence times of 1 minuteto 5 minutes.

In another mode, an aqueous slurry comprising the desired formulationingredients is sprayed into a fluidized bed of particulate surfactants.The resulting particles can be further densified by passage through aLodige apparatus, as noted above. The perfume delivery particles areadmixed with the detergent composition in the Lodige apparatus.

The final density of the particles herein can be measured by a varietyof simple techniques, which typically involve dispensing a quantity ofthe granular detergent into a container of known volume, measuring theweight of detergent and reporting the density in grams/liter.

Once the low or high density granular detergent “base” composition isprepared, the encapsulated perfume particles of this invention are addedthereto by any suitable dry-mixing operation.

Deposition of Perfume Onto Fabric Surfaces

The method of washing fabrics and depositing perfume thereto comprisescontacting said fabrics with an aqueous wash liquor comprising at leastabout 100 ppm of conventional detersive ingredients describedhereinabove, as well as at least about 0.1 ppm of the above-disclosedencapsulated perfume particles. Preferably, the aqueous liquor comprisesfrom about 500 ppm to about 20,000 ppm of the conventional detersiveingredients and from about 10 ppm to about 200 ppm of the encapsulatedperfume particles.

The encapsulated perfume particles work under all wash conditions, butthey are particularly useful for providing odor benefits to the wetlaundry solution during use and on dried fabrics during their storage.

The following nonlimiting examples illustrate the parameters of andcompositions employed within the invention. All percentages, parts andratios are by weight unless otherwise indicated.

Components 5 6 7 8 9 10 11 LAS 21.6 18 25 5 0 18 22 AES 1.0 1.5 — — —1.0 — ADHQ 0.7 0.6 — — — 0.6 — AE — 0.4 0.5 — — — 0.9 Phosphate 22 13 212 — 22 21 Silicate 7.5 7.5 10 — — 7.5 3.5 Carbonate 13 9 10 80 70 13 4.5Zeolite — 1.5 — — — — — DTPA 0.9 0.9 — — — 0.9 — SOKALAN ® 1.0 0.9 — — —1.0 — PEI 1800 E₇ — — — — — — — CMC 0.6 0.35 — — — 0.60 0.25 SRA-1 0.20.2 — — — 0.2 — Protease/amylase 0.36 0.54 0.3 — — 0.36 0.5 Cellulase007 0.07 — — — 0.07 0.1 Lipase — — 0.05 — — — — Perborate 4.10 1.35 —4.0 — 2.25 — NOBS 1.70 1.15 — — — 1.90 — TEAD 0.6 — — — — 0 — ZPS 0.00150.007 — — — 0.0015 — Brighteners 0.2 0.04 0.15 — — 0.2 0.03 EncapsulatedHIA 0.8 0.8 0.8 0.8 0.8 0.8 0.8 Perfume particle from Example 1Moisture + spray- 6.0 5.6 8.9 6.0 5.9 6.0 6.0 on perfume Sulfate balancebalance balance balance balance balance Balance

What is claimed is:
 1. An encapsulated perfume particle comprising: a) awater-soluble modified starch solid matrix, wherein the modified starchcomprises a starch raw material that has been modified by treatment ofthe starch raw material with octenyl-succinic acid anyhydride; b) aperfume oil encapsulated by the solid matrix of the modified starch,comprising at least 40% by weight of at least 2 High Impact Accord(“HIA”) perfume ingredients, each of said perfume ingredient having (1)a boiling point at 760 mm Hg, of 275° C. or lower, (2) a calculatedCLogP of 2.0 or higher, and (3) an odor detection threshold (“ODT”) lessthan or equal to 50 ppb and greater than 10 ppb; wherein the perfumeparticle begins to release the encapsulated perfume immediately uponaddition to water.
 2. An encapsulated perfume particle according toclaim 1, wherein the perfume oil comprises at least 50%, of said HIAperfume ingredients.
 3. An encapsulated perfume particle according toclaim 1, wherein the perfume oil comprises at least 70% of said HIAperfume ingredients.
 4. A granular detergent composition comprising: I)from about 0.01% to about 50%, by weight, of an encapsulated perfumeparticle comprising; (a) a water-soluble modified starch solid matrix;(b) a perfume oil comprising at least 40% by weight of at least 2 HighImpact Accord (“HIA”) perfume ingredients, each said HIA perfumeingredient having (1) a boiling point at 760 mm Hg, of 275° C. or lower,(2) a calculated CLogP of 2.0 or higher, and (3) an odor detectionthreshold (“ODT”) less than or equal to 50 ppb and greater than 10 ppband; II) from about 50% to about 99.99%, of conventional laundryingredients selected from the group consisting of surfactants, builders,bleaching agents, enzymes, soil release polymers, dye transferinhibitors, fillers, and mixtures thereof.
 5. A granular detergentcomposition according to claim 4 wherein the composition comprises fromabout 0.05% to about 8.0%, by weight, of the encapsulated perfumeparticle, wherein the perfume oil comprises at least 50%, of said HIAperfume ingredients and from about 92% to about 99.95%, of saidconventional laundry ingredients.
 6. A granular detergent compositionaccording to claim 4 wherein the composition comprises from about 0.05%to 3.0%, by weight, of the encapsulated perfume particle, wherein theperfume oil comprises at least 50% of said HIA perfume ingredients andfrom about 97% to about 99.95%, of said conventional laundryingredients.
 7. A granular detergent composition according to claim 4wherein the composition comprises from about 0.05% to 1.0% by weight, ofthe encapsulated perfume particle, wherein the perfume oil comprises atleast 50%, of said HIA perfume ingredients and from about 99% to about99.95% of said conventional laundry ingredients.
 8. A detergentcomposition according to claim 4 further comprising a perfume sprayedonto the surface of said detergent composition.
 9. A detergentcomposition according to claim 5 further comprising a perfume sprayedonto the surface of said detergent composition.
 10. A detergentcomposition according to claim 6 further comprising a perfume sprayedonto the surface of said detergent composition.
 11. A detergentcomposition according to claim 7 further comprising a perfume sprayedonto the surface of said detergent composition.